Triethylamine → HCID 86655165, compound

Participants

Reaction Conditions

Reaction Steps

500 mg of 2-cyano-3,5-difluoropyridine, 426 mg of 2-fluoroethylamine hydrochloride, 987 mg of potassium carbonate and 433 mg of triethylamine in 10 ml of dimethyl sulphoxide are introduced into a 20 ml microwave tube reactor. The mixture is then heated in the microwave for 1 and a half hours at 115° C. The reaction medium is run into 100 ml of water and 100 ml of ethyl acetate. The aqueous phase is re-extracted twice with 50 ml with ethyl acetate. The combined organic phases are washed with water and then with a saturated aqueous solution of sodium chloride, dried over sodium sulphate and concentrated under reduced pressure. After purification by flash chromatography on 70 g of silica gel, elution being carried out with a mixture of ethyl acetate and cyclohexane (30/70 by volume), and the first eluted product being recovered, 125 mg of 2-cyano-5-fluoro-3-(2-fluoroethylamino)pyridine are thus obtained in the form of a white powder, the characteristics of which are the following:

Provenance & Evidence